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A kind of preparation method of bio-based polyester

A technology based on polyester and biology, which is applied in the field of preparation of bio-based polyester to achieve the effect of eliminating depolymerization and controllable polymerization.

Active Publication Date: 2022-03-11
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of organic small molecule catalysts to control polycondensation reactions has not been reported at home and abroad.

Method used

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  • A kind of preparation method of bio-based polyester
  • A kind of preparation method of bio-based polyester
  • A kind of preparation method of bio-based polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] For the preparation of DBU·BA, dissolve benzoic acid in ether solution at room temperature under nitrogen or inert gas protection conditions, and drop DBU into the reaction flask while stirring to obtain the product. The hydrogen spectrum structure of DBU·BA is as follows figure 1 As shown, the carbon spectrum structure is as figure 2 shown.

[0035] The argon in the reaction kettle was replaced three times, and 19.4g of dimethyl terephthalate and 10.8ml of ethylene glycol (molar ratio of 1:2) were added under the state of argon, and the temperature was gradually raised to 250 ℃, carry out the condensation reaction until no methanol is distilled out. Add 0.028g DBU·BA salt (0.1% mol) and reduce the pressure to 0.3 atmosphere to carry out the transesterification reaction, raise the temperature to 280°C until no ethylene glycol evaporates. After the reaction was complete, cool to room temperature with nitrogen gas, and the product was a colorless transparent solid wit...

Embodiment 2

[0037] The DBU·BA catalyst was prepared as in Example 1.

[0038] Replace the argon in the reaction kettle three times, add 19.4g dimethyl terephthalate and 14.5ml 1,3-propanediol (molar ratio is 1:2) under the state of argon, and gradually increase the temperature under normal pressure To 250 ° C, the condensation reaction is carried out until no methanol is distilled out. Then add 0.028g of DBU·BA salt (0.1% mol), then reduce the pressure to 0.2 atmosphere to carry out the transesterification reaction, raise the temperature to 280°C until no ethylene glycol is distilled out. After the reaction was complete, the reaction was cooled to room temperature with nitrogen gas, and the product was a colorless transparent solid with a weight of 19.9 g and a yield of 60%.

Embodiment 3

[0040] The DBU·BA catalyst was prepared as in Example 1.

[0041] The argon in the reaction kettle was pumped three times, and 19.4g of dimethyl terephthalate and 17.7ml of 1,4-butanediol (molar ratio was 1:2) were added under the state of argon, and gradually increased under normal pressure. The temperature is up to 220°C, and the condensation reaction is carried out until no methanol is distilled out. Then add 1.12g of DBU·BA salt (4% mol), then reduce the pressure to 0.3 atmospheric pressure to carry out the transesterification reaction, raise the temperature to 280°C until no ethylene glycol evaporates. After the reaction is complete, the nitrogen gas is cooled to room temperature, and the product is a colorless, transparent to pale yellow solid, with a product weight of 25.3 g and a yield of 65%. The product PBT and its raw materials are as follows: Figure 4 shown.

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Abstract

The technical field of organic synthesis of the present invention particularly relates to a preparation method of bio-based polyester. The invention adopts a two-step method to synthesize terephthalic acid and its derivatives into high molecular weight polyester compounds. Adopt the method of the present invention, realize efficient, gentle, controllable polymerization reaction, completely avoid introducing any metal in the catalytic polymerization reaction process, and put an end to the depolymerization reaction of the catalyst in the secondary (or follow-up) process, and construct the polymerization of predetermined structure Molecules to realize the design and control of the properties of polymer materials.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of bio-based polyester. Background technique [0002] With the increasingly serious problems of environmental protection and fossil resources, the development of bio-based polymer materials based on renewable biomass resources has become a future development trend. As one of the most valuable bio-based platform compounds, terephthalic acid and its derivatives have been widely attempted in the synthesis of fine chemicals and polymer materials. [0003] In recent years, for metal catalyst systems, tin-containing metal series catalysts represented by stannous isooctanoate (SnOct2) are the most commonly used catalyst types for ring-opening polymerization. In the earliest research of Carothers and the current industrial production, tin-based, bismuth-based and antimony-based compounds are commonly used as polycondensation catalysts. In the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/87C08G63/183
CPCC08G63/87C08G63/183
Inventor 郭凯姚志威李振江张婵朱玥嘉张磊罗子堃高宇王海鑫颜蕊
Owner NANJING TECH UNIV
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